CN105294934A - High-intensity and antibacterial hydrogel and preparation method thereof - Google Patents
High-intensity and antibacterial hydrogel and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a preparation method of high-intensity and antibacterial hydrogel. The method comprises the steps of dissolving maleic acid, acrylamide, carboxymethyl chitosan, a cross-linking agent, an initiator and a catalyst in an aqueous solution by using cooled boiled distilled water, rapidly transferring the prepared solution into a glass mold, placing the sealed mold under an environment of 45 to 55 DEG C and performing a heat preservation reaction for 2 to 6 hours; then taking out formed hydrogel in the mold, soaking in a soluble metal salt solution with the concentration of 0.05 to 0.25 M for 24 hours, afterwards, taking out the high-intensity and antibacterial hydrogel. The hydrogel disclosed by the invention has a good antibacterial effect while performing certain mechanical strength, so as to meet the application demand of the hydrogel in the aspects of human body cartilage repair, tissue engineering and the like.
Description
Technical field
The present invention relates to a kind of preparation field of hydrogel, especially the preparation of high strength, high antibacterial performance hydrogel.
Technical background
Hydrogel is the one of functional high molecule material, and thus inner have special adsorption to water with strong hydrophilic radical, by intermolecular cross-linking, forms reticulated structure.The feature of water-absorbent gelatinous material water suction is different from the sorbing material such as sponge, cotton, and it can absorb is the water of sole mass hundreds and thousands of times, and with water mortise, then expand and form hydrogel.Also be seldom extruded even if the water in this gel is subject to sizable pressure.This specific function makes absorbent polymer gelatinous material just be developed rapidly after being found.Prepare hydrogel and generally adopt macromolecular material, comprise natural macromolecular material and synthesized polymer material.Natural macromolecular material because of its biocompatibility better and often selected, but also there are some shortcomings in natural polymer: the poor repeatability of such as material property, physical strength is poor, and Structure and Properties variable range is narrow, causes it to be difficult to meet its various actual requirement.Synthesis macromolecule hydrogel has plurality of advantages: synthetic materials is by control condition, and its production is reproducible, can produce in a large number as required, by simple physics, chemical modification, obtains performance widely, with satisfied different needs.But it is generally poor to synthesize high molecular biocompatibility.In order to solve the problem, increasing investigator has attempted the hydrogel that various method removes synthesizing new.JournalofPolymerScience periodical had such one section of report in 2004, the people such as the Park polyvinyl alcohol/polyvidone copolymer aquagel that adopted freeze-thaw method to synthesize, the effect that aloe composition has reached antibacterial is added in building-up process, found the increase along with aloe content in polymkeric substance afterwards, the strength degradation of gel.Therefore make and a kind ofly there is the hydrogel that certain physical strength has a good germ resistance simultaneously there is very large practical application meaning and prospect.
Cm-chitosan (CMCH) is a kind of water-solubility chitosan derivative, has numerous characteristics, and as germ resistance is strong, having freshening effect, is a kind of polyamphoteric electrolyte etc.Makeup, fresh-keeping, medical etc. in have multiple application, be also that Recent study obtains one of more chitosan derivatives.In addition, maleic acid (MA) is a kind of polymer monomer containing two carboxyls and a unsaturated double-bond, copolymerization can be produced with other monomers containing double bond when retaining carboxyl, due to containing a large amount of carboxyl on macromole long-chain after copolymerization, thus ionic linkage can be formed with metallic cation, strengthen the physical strength of polymkeric substance.
The domestic research for high strength anti-bacterial hydrogel and report considerably less, this is because general hydrogel is difficult to accomplish that high strength and good antimicrobial property are taken into account simultaneously, and there are some defects in many hydrogels itself, the problems such as the infection that bacterium causes as contacted, some medical aquogel does not have anti-microbial property due to itself, therefore in use must by various mode sterilizings etc.Maleic acid, acrylamide (AM) and cm-chitosan are reacted by catalyzer, initiator and linking agent by the present invention in aqueous, then constructed a kind of simultaneously containing Semi-IPN double-network hydrogel that is covalently cross-linked and ionic crosslinking by the method for metallic cation immersion treatment, this hydrogel product has possessed good antibacterial effect while showing certain physical strength.
Summary of the invention
For preparing a kind of novel high-strength anti-bacterial hydrogel, maleic acid, acrylamide and cm-chitosan are reacted by catalyzer, initiator and linking agent by the present invention in aqueous, are then constructed a kind of simultaneously containing Semi-IPN double-network hydrogel that is covalently cross-linked and ionic crosslinking successively by the method for metallic cation immersion treatment.Prepared high intensity hydrogel tension strain can reach 162%, and tensile strength can reach 1.44MPa, and energy-to-break can reach 62.48MJ/m
3.
Interpenetrating net polymer is the aggregated structure that two kinds of polymkeric substance run through mutually with the form of network, in interpenetrating net polymer, have at least a kind of polymkeric substance to be synthesizing cross-linked, another kind of polymkeric substance and front a kind of polymkeric substance do not have covalent bonds, but among the network of front a kind of polymkeric substance.Wherein Semi-IPNly refer in the network by two kinds of polymer formation, if there is one to be linear molecule, this network is called semiinterpenetrating polymer network; Double-network hydrogel refers to the hydrogel be made up of two IPNs or Semi-IPN polymer network, and they are better than wherein any one single network gel on mechanical strength and toughness.In dual network gel, the segment of one of them network is in highly unfolds and closely knit crosslinked state, gives gel-strength and rigidity; The segment of another network is then in curls and loose crosslinked state, makes gel have flexibility and toughness.
In order to achieve the above object, the technical solution used in the present invention is as follows:
The invention provides a kind of novel high-strength anti-bacterial hydrogel, it is characterized in that, there is following chain unit:
Wherein mass ratio and the maleic acid of each structural unit, acrylamide are identical with the feed ratio of linking agent, i.e. m:n:t=MA (maleic acid): AM (acrylamide): linking agent (quality, with reference to each embodiment);
Preferably, described high strength anti-bacterial hydrogel, is characterized in that, this hydrogel belongs to build and is cross-linked, and whole gel is a macromole in theory, and the quality of an one molecule equals the quality of whole gel;
Preferably, described high strength anti-bacterial hydrogel, is characterized in that, its infrared spectra has the charateristic avsorption band of following wavelength:
3347 ~ 33493,3196 ~ 3198,2936 ~ 2938,1658 ~ 1660,1416 ~ 1418,1323 ~ 1325,1119 ~ 1121,691 ~ 693; Its infrared spectra as shown in Figure 5.
Preferably, the tension strain of described high strength anti-bacterial hydrogel is 50 ~ 250%, and tensile strength is 0 ~ 3MPa, energy-to-break 30 ~ 70MJ/m
3;
Preferably, described high strength anti-bacterial hydrogel, is prepared from by each component of following weight parts:
Maleic acid 0.5 ~ 2.5 part, acrylamide 4 ~ 6 parts, cm-chitosan 0.5 ~ 2 part, soluble metallic salt 0.05 ~ 0.25 part, linking agent, initiator, catalyzer are respectively 0.02 ~ 0.08wt%, 0.11 ~ 0.21wt%, the 0.18 ~ 0.3wt% of maleic acid, acrylamide and the total number of cm-chitosan three;
Described linking agent is selected from Ethylene glycol dimethacrylate, N, N '-methylene-bisacrylamide, wherein a kind of in Vinylstyrene;
Described initiator is selected from the wherein one in Potassium Persulphate, ammonium persulphate, Sodium Persulfate;
Described catalyzer is selected from the wherein one in five methyl diethylentriamine, Tetramethyl Ethylene Diamine;
Described soluble metallic salt is selected from FeCl
3, AlCl
3, CaCl
2, MgCl
2in wherein a kind of.
The present invention also provides the preparation method of described hydrogel, it is characterized in that, comprises the following steps:
1) distilled water is boiled sealing and be cooled to room temperature with except the oxygen in anhydrating, cooled water is for subsequent use;
2) vacuumize and under Keep agitation condition, get maleic acid, acrylamide and cm-chitosan and be dissolved in step 1) in the water prepared, described maleic acid 0.5 ~ 2.5 part, acrylamide 4 ~ 6 parts, cm-chitosan 0.5 ~ 2 part;
3) under vacuum, Keep agitation condition, linking agent, initiator, catalyzer are added step 2) in the solution of gained, continue stirring until solution transparent, after suspending without solid particulate, stopping vacuumizes, and described linking agent, initiator, catalyzer are respectively 0.02 ~ 0.08wt%, 0.11 ~ 0.21wt%, the 0.18 ~ 0.3wt% of maleic acid, acrylamide and the total number of cm-chitosan three;
4) by step 3) solution for preparing is transferred in glass mold, and after sealing, at being placed in 45 ~ 55 DEG C, insulation reaction 4 ~ 6h, is shaping hydrogel;
5) hydrogel being immersed in concentration is in the soluble metal salt brine solution of 0.05 ~ 0.25M 24 hours, takes out hydrogel and continues to soak 24 hours in deionized water, obtain product.
Preferably, described vacuum is the vacuum tightness of-0.1 ~ 0MPa.
Maleic acid and acrylamide copolymerization in the present invention by covalently cross-linked formation macromolecular network together with the cm-chitosan macromolecular chain IPN in solution, then, after hydrogel is soaked by metal cation solution, the carboxyl on cm-chitosan macromolecular chain, the carboxyl on maleic acid and metallic cation form the intensity that ionic linkage further enhances again this hybrid network.
In the process building ionic crosslinking, we have selected maleic acid as the polymerization single polymerization monomer with reactive behavior point.Maleic acid is compared to the carboxyl that vinylformic acid has two times of equivalents can improve more cross-linking set, simultaneously because vinylformic acid has stronger corrodibility and toxicity, adopts maleic acid to substitute vinylformic acid and can reduce potential hazard in production process.
Beneficial effect of the present invention:
1, the present invention adopts form that is covalently cross-linked and ionic crosslinking simultaneously, build a kind of Semi-IPN double network polymer hydrogel, because covalently cross-linked hydrogel automatic recovery ability is poor, after using ionic linkage to have fracture, the autonomous characteristic recovered can improve the automatic recovery ability of this hydrogel effectively.
2, the present invention adopts cm-chitosan to be reactant, at the carboxyl utilized on cm-chitosan molecular chain and Fe
3+ion is formed while ionic crosslinking, the character utilizing itself stable and antibacterial anti-infection performance, this hydrogel is possessed simultaneously stronger mechanical property and good antimicrobial property.
3, present invention employs maleic acid as the polymer monomer building ionic crosslinking, on the basis of hydrogel taking vinylformic acid as reaction monomers, solve the toxicity that Acrylic Acid Monomer brings, corrosive harm, maleic acid has can providing more cross-linking set for network thus increase network strength of two times of equivalents simultaneously.
In sum, the hydrogel of the high strength prepared of the present invention and anti-microbial property has the advantages such as preparation method is simple effectively, mechanical strength is large, anti-microbial property is good.
Accompanying drawing explanation
Fig. 1, Fig. 2 are the stress-strain curve of the high intensity hydrogel sample extension experiment of the embodiment of the present invention 1 ~ 6 gained.
Fig. 3, Fig. 4 are the antibacterial experiment figure of the high intensity hydrogel sample of the embodiment of the present invention 4 ~ 8 gained.
Fig. 5 is the infared spectrum of the high intensity hydrogel sample of the embodiment of the present invention 2 gained.
Embodiment
For making those skilled in the art understand the present invention better, the preparation method of the novel hydrogels possessing superelevation mechanical strength and chemical stability is described in the application below by way of specific embodiment.
Embodiment 1
1) distilled water is boiled sealing and be cooled to room temperature with except the oxygen in anhydrating, cooled water is for subsequent use;
2) be evacuated to-0.1MPa and under Keep agitation condition, get maleic acid, acrylamide and cm-chitosan and be dissolved in step 1) in the water prepared, described maleic acid 2.25 parts, acrylamide 5 parts, cm-chitosan 0.75 part;
3) under vacuum (-0.1MPa), Keep agitation condition, linking agent, initiator, catalyzer are added step 2) in the solution of gained, continue stirring until solution transparent, after suspending without solid particulate, stopping vacuumizes, and described linking agent, initiator, catalyzer are respectively 0.06wt%, 0.16wt%, 0.24wt% of maleic acid, acrylamide and the total number of cm-chitosan three;
4) by step 3) solution for preparing is transferred in glass mold, and after sealing, at being placed in 55 DEG C, insulation reaction 5h, is shaping hydrogel;
5) hydrogel being immersed in concentration is 24h in the soluble metal salt brine solution of 0.15M, takes out hydrogel and continues to soak 24h in deionized water, obtain product.
The high intensity hydrogel product called after 30%MA/AM/10%CMCH that the present embodiment obtains, its tension strain can reach 109%, and tensile strength can reach 1.45MPa.
Embodiment 2
1) distilled water is boiled sealing and be cooled to room temperature with except the oxygen in anhydrating, the cooled aqueous solution is for subsequent use;
2)-0.1MPa is evacuated to and under Keep agitation condition, get maleic acid, acrylamide and cm-chitosan and be dissolved in step 1) in the water prepared, described maleic acid 1.5 parts, acrylamide 5.25 parts, cm-chitosan 0.75 part;
3) under vacuum (-0.1MPa), Keep agitation condition, linking agent, initiator, catalyzer are added step 2) in the solution of gained, continue stirring until solution transparent, after suspending without solid particulate, stopping vacuumizes, and described linking agent, initiator, catalyzer are respectively 0.06wt%, 0.16wt%, 0.24wt% of maleic acid, acrylamide and the total number of cm-chitosan three;
4) by step 3) solution for preparing is transferred in glass mold, and after sealing, at being placed in 55 DEG C, insulation reaction 5h, is shaping hydrogel;
5) hydrogel being immersed in concentration is 24h in the soluble metal salt brine solution of 0.15M, takes out hydrogel and continues to soak 24h in deionized water, obtain product.
The high intensity hydrogel product called after 20%MA/AM/10%CMCH that the present embodiment obtains, its tension strain can reach 162%, and tensile strength can reach 1.44MPa.
Embodiment 3
1) distilled water is boiled sealing and be cooled to room temperature with except the oxygen in anhydrating, the cooled aqueous solution is for subsequent use;
2) be evacuated to-0.1MPa and under Keep agitation condition, get maleic acid, acrylamide and cm-chitosan and be dissolved in step 1) in the water prepared, described maleic acid 0.75 part, acrylamide 6 parts, cm-chitosan 0.75 part;
3) under vacuum (-0.1MPa), Keep agitation condition, linking agent, initiator, catalyzer are added step 2) in the solution of gained, continue stirring until solution transparent, after suspending without solid particulate, stopping vacuumizes, and described linking agent, initiator, catalyzer are respectively 0.06wt%, 0.16wt%, 0.24wt% of maleic acid, acrylamide and the total number of cm-chitosan three;
4) by step 3) solution for preparing is transferred in glass mold, and after sealing, at being placed in 55 DEG C, insulation reaction 5h, is shaping hydrogel;
5) hydrogel being immersed in concentration is 24h in the soluble metal salt brine solution of 0.15M, takes out hydrogel and continues to soak 24h in deionized water, obtain product.
The high intensity hydrogel product called after 10%MA/AM/10%CMCH that the present embodiment obtains, its tension strain can reach 152%, and tensile strength can reach 0.74MPa.
Embodiment 4
1) distilled water is boiled sealing and be cooled to room temperature with except the oxygen in anhydrating, the cooled aqueous solution is for subsequent use;
2)-0.1MPa is evacuated to and under Keep agitation condition, get maleic acid, acrylamide and cm-chitosan and be dissolved in step 1) in the water prepared, described maleic acid 1.5 parts, acrylamide 5.25 parts, cm-chitosan 0.75 part;
3) under vacuum (-0.1MPa), Keep agitation condition, linking agent, initiator, catalyzer are added step 2) in the solution of gained, continue stirring until solution transparent, after suspending without solid particulate, stopping vacuumizes, and described linking agent, initiator, catalyzer are respectively 0.06wt%, 0.16wt%, 0.24wt% of maleic acid, acrylamide and the total number of cm-chitosan three;
4) by step 3) solution for preparing is transferred in glass mold, and after sealing, at being placed in 55 DEG C, insulation reaction 5h, is shaping hydrogel;
5) hydrogel being immersed in concentration is 24h in the soluble metal salt brine solution of 0.15M, takes out hydrogel and continues to soak 24h in deionized water, obtain product.
The high intensity hydrogel product called after 10%CMCH/AM/20%MA that the present embodiment obtains, its tension strain can reach 162%, and tensile strength can reach 1.44MPa.
Embodiment 5
1) distilled water is boiled sealing and be cooled to room temperature with except the oxygen in anhydrating, the cooled aqueous solution is for subsequent use;
2)-0.1MPa is evacuated to and under Keep agitation condition, get maleic acid, acrylamide and cm-chitosan and be dissolved in step 1) in the water prepared, described maleic acid 1.5 parts, acrylamide 4.875 parts, cm-chitosan 1.125 parts;
3) under vacuum (-0.1MPa), Keep agitation condition, linking agent, initiator, catalyzer are added step 2) in the solution of gained, continue stirring until solution transparent, after suspending without solid particulate, stopping vacuumizes, and described linking agent, initiator, catalyzer are respectively 0.06wt%, 0.16wt%, 0.24wt% of maleic acid, acrylamide and the total number of cm-chitosan three;
4) by step 3) solution for preparing is transferred in glass mold, and after sealing, at being placed in 55 DEG C, insulation reaction 5h, is shaping hydrogel;
5) hydrogel being immersed in concentration is 24h in the soluble metal salt brine solution of 0.15M, takes out hydrogel and continues to soak 24h in deionized water, obtain product.
The high intensity hydrogel product called after 15%CMCH/AM/20%MA that the present embodiment obtains, its tension strain can reach 102%, and tensile strength can reach 1.34MPa.
Embodiment 6
1) distilled water is boiled sealing and be cooled to room temperature with except the oxygen in anhydrating, the cooled aqueous solution is for subsequent use;
2) be evacuated to-0.1MPa and under Keep agitation condition, get maleic acid, acrylamide and cm-chitosan and be dissolved in step 1) in the water prepared, described maleic acid 1.5 parts, acrylamide 4.5 parts, cm-chitosan 1.5 parts;
3) under vacuum (-0.1MPa), Keep agitation condition, linking agent, initiator, catalyzer are added step 2) in the solution of gained, continue stirring until solution transparent, after suspending without solid particulate, stopping vacuumizes, and described linking agent, initiator, catalyzer are respectively 0.06wt%, 0.16wt%, 0.24wt% of maleic acid, acrylamide and the total number of cm-chitosan three;
4) by step 3) solution for preparing is transferred in glass mold, and after sealing, at being placed in 55 DEG C, insulation reaction 5h, is shaping hydrogel;
5) hydrogel being immersed in concentration is 24h in the soluble metal salt brine solution of 0.15M, takes out hydrogel and continues to soak 24h in deionized water, obtain product.
The high intensity hydrogel product called after 20%CMCH/AM/20%MA that the present embodiment obtains, its tension strain can reach 81%, and tensile strength can reach 1.36MPa.
Embodiment 7
1) distilled water is boiled sealing and be cooled to room temperature with except the oxygen in anhydrating, the cooled aqueous solution is for subsequent use;
2) be evacuated to-0.1MPa and under Keep agitation condition, get maleic acid and acrylamide is dissolved in step 1) in the water prepared, described maleic acid 1.5 parts, acrylamide 6 parts;
3) under vacuum (-0.1MPa), Keep agitation condition, linking agent, initiator, catalyzer are added step 2) in the solution of gained, continue stirring until solution transparent, after suspending without solid particulate, stopping vacuumizes, and described linking agent, initiator, catalyzer are respectively 0.06wt%, 0.16wt%, 0.24wt% of the total number of both maleic acid and acrylamide;
4) by step 3) solution for preparing is transferred in glass mold, and after sealing, at being placed in 55 DEG C, insulation reaction 5h, is shaping hydrogel;
5) hydrogel being immersed in concentration is 24h in the soluble metal salt brine solution of 0.15M, takes out hydrogel and continues to soak 24h in deionized water, obtain product.
The high intensity hydrogel product called after 20%MA/AM that the present embodiment obtains, its tension strain can reach 275.8%, and tensile strength can reach 1.25MPa.
Embodiment 8
1) distilled water is boiled sealing and be cooled to room temperature with except the oxygen in anhydrating, the cooled aqueous solution is for subsequent use;
2)-0.1MPa is evacuated to and under Keep agitation condition, get maleic acid, acrylamide and cm-chitosan and be dissolved in step 1) in the water prepared, described maleic acid 1.5 parts, acrylamide 5.25 parts, cm-chitosan 0.75 part;
3) under vacuum (-0.1MPa), Keep agitation condition, linking agent, initiator, catalyzer are added step 2) in the solution of gained, continue stirring until solution transparent, after suspending without solid particulate, stopping vacuumizes, and described linking agent, initiator, catalyzer are respectively 0.06wt%, 0.16wt%, 0.24wt% of maleic acid, acrylamide and the total number of cm-chitosan three;
4) by step 3) solution for preparing is transferred in glass mold, and after sealing, at being placed in 55 DEG C, insulation reaction 5h, is shaping hydrogel, obtains product.
The high intensity hydrogel product that the present embodiment obtains is cross-linked owing to not having iron ion, has extremely low tensile strength and high elongation at break, exceeds surveyed universal testing machine scope, therefore tensionless winkler foundation data.
Experimental example
Stratographic analysis: at the absorption peak of wavelength to be 3348.6 and 3197.3 positions be O-H and N-H, the absorption peak of wavelength to be 2937.0 positions be C-H, wavelength is 1659.8 positions is C=O absorption peaks, wavelength is 1417.6 positions is C-H absorption peaks, the absorption peak of wavelength to be 1324.0 and 1120.3 positions be C-O, the absorption peak of wavelength to be 692.3 positions be C-H.Its infrared spectra as shown in Figure 5.
Elongation test: adopt universal testing machine (LR10KPlus) to carry out Elongation test to the sheet-like hydrous gel sample that length, width, thickness are respectively 50mm, 10mm, 3mm, gauge length is 10mm, and rate of extension is 50mm/min.Same sample test three times, test result is averaged.In embodiment 1,2,3,4,5,6, gained sample extension test result as shown in Figure 1 and Figure 2.
Antibacterial test: respectively the hydrogel of embodiment 4 ~ 8 is made cylindric, stand-by; Take out the streptococcus aureus bacterium liquid that 18h cultivated by shaking table, then in aseptic operating platform, draw 100uL streptococcus aureus with liquid-transfering gun respectively and beat on nutrient agar plate, then with spreader, bacterium liquid is coated with evenly.Then the dull and stereotyped circle centre position hydrogel of embodiment 4 ~ 8 put into.The flat board being placed with sample is just being placed to constant incubator carry out cultivating about 18h.To kill the scope radius of neighbouring bacterium for measurement index.In embodiment 4,5,6,7,8, gained sample anti-bacteria test result as shown in Figure 3, Figure 4.Detected result shows: this hydrogel has powerful killing effect to streptococcus aureus.
The dead scope radius of table 1. culturing bacterium
Claims (1)
1. the invention provides a kind of novel high-strength anti-bacterial hydrogel, it is characterized in that, there is following chain unit:
Wherein mass ratio and the maleic acid of each structural unit, acrylamide are identical with the feed ratio of linking agent, i.e. m:n:t=MA (maleic acid): AM (acrylamide): linking agent (quality, with reference to each embodiment);
Preferably, described high strength anti-bacterial hydrogel, is characterized in that, this hydrogel belongs to build and is cross-linked, and whole gel is a macromole in theory, and the quality of an one molecule equals the quality of whole gel;
Preferably, described high strength anti-bacterial hydrogel, is characterized in that, its infrared spectra has the charateristic avsorption band of following wavelength:
3347 ~ 33493,3196 ~ 3198,2936 ~ 2938,1658 ~ 1660,1416 ~ 1418,1323 ~ 1325,1119 ~ 1121,691 ~ 693; Its infrared spectra as shown in Figure 5.
Preferably, the tension strain of described high strength anti-bacterial hydrogel is 50 ~ 250%, and tensile strength is 0 ~ 3MPa, energy-to-break 30 ~ 70MJ/m
3;
Preferably, described high strength anti-bacterial hydrogel, is prepared from by each component of following weight parts:
Maleic acid 0.5 ~ 2.5 part, acrylamide 4 ~ 6 parts, cm-chitosan 0.5 ~ 2 part, soluble metallic salt 0.05 ~ 0.25 part, linking agent, initiator, catalyzer are respectively 0.02 ~ 0.08wt%, 0.11 ~ 0.21wt%, the 0.18 ~ 0.3wt% of maleic acid, acrylamide and the total number of cm-chitosan three;
Described linking agent is selected from Ethylene glycol dimethacrylate, N, N '-methylene-bisacrylamide, wherein a kind of in Vinylstyrene;
Described initiator is selected from the wherein one in Potassium Persulphate, ammonium persulphate, Sodium Persulfate;
Described catalyzer is selected from the wherein one in five methyl diethylentriamine, Tetramethyl Ethylene Diamine;
Described soluble metallic salt is selected from FeCl
3, AlCl
3, CaCl
2, MgCl
2in wherein a kind of.
The present invention also provides the preparation method of described hydrogel, it is characterized in that, comprises the following steps:
1) distilled water is boiled sealing and be cooled to room temperature with except the oxygen in anhydrating, cooled water is for subsequent use;
2) vacuumize and under Keep agitation condition, get maleic acid, acrylamide and cm-chitosan and be dissolved in step 1) in the water prepared, described maleic acid 0.5 ~ 2.5 part, acrylamide 4 ~ 6 parts, cm-chitosan 0.5 ~ 2 part;
3) under vacuum, Keep agitation condition, linking agent, initiator, catalyzer are added step 2) in the solution of gained, continue stirring until solution transparent, after suspending without solid particulate, stopping vacuumizes, and described linking agent, initiator, catalyzer are respectively 0.02 ~ 0.08wt%, 0.11 ~ 0.21wt%, the 0.18 ~ 0.3wt% of maleic acid, acrylamide and the total number of cm-chitosan three;
4) by step 3) solution for preparing is transferred in glass mold, and after sealing, at being placed in 45 ~ 55 DEG C, insulation reaction 4 ~ 6h, is shaping hydrogel;
5) hydrogel being immersed in concentration is in the soluble metal salt brine solution of 0.05 ~ 0.25M 24 hours, takes out hydrogel and continues to soak 24 hours in deionized water, obtain product.
Preferably, described vacuum is the vacuum tightness of-0.1 ~ 0MPa.
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|---|---|---|---|---|
| CN111138582A (en) * | 2020-01-10 | 2020-05-12 | 中国科学院大学温州研究院(温州生物材料与工程研究所) | Anionic polymer hydrogel containing copper ions as well as preparation method and application of anionic polymer hydrogel |
| CN115845122A (en) * | 2021-09-23 | 2023-03-28 | 齐鲁工业大学 | Photosensitive and temperature-sensitive mixed type high-strength hydrogel |
| CN115845122B (en) * | 2021-09-23 | 2024-02-02 | 齐鲁工业大学 | Photosensitive and temperature-sensitive mixed high-strength hydrogel |
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